Specimen Preparation


Specimen preparation is a very broad subject; there are books devoted to this topic alone. The intention here is to summarize the techniques, suggest routes that you might follow, and above all to emphasize that there are many ways to produce a TEM specimen; the one you choose will depend on the information you need, time constraints, availability of equipment, your skill, and the material. So we’ll concentrate on the ‘principles of cooking,’ but won’t try to list all the possible ‘recipes.’ One important point to bear in mind is that your technique must not affect what you see or measure, or if it does, then you must know how. Specimen preparation artifacts may be interesting but they are not usually what you want to study. Incidentally, we’ll make ‘specimens’ from the ‘sample’ we’re investigating so we’ll look at ‘TEM specimens,’ but sometimes we, and everyone else, will interchange the two words.


Specimen Preparation Safety Data Sheet Electron Transparency Irregular Topography Etch Stop 
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  1. These references only give a sampling. More extensive lists, especially for the more specialized techniques like FIB, are given in the companion text.Google Scholar

General Techniques

  1. An extensive list of references is included in the chapter on specimen preparation in the companion text. The first four references below are essential: from the MRS Proceedings.Google Scholar
  2. i. Bravman, JC, Anderson, RM and McDonald, ML (Eds.) 1988 Specimen Preparation for Transmission Electron Microscopy of Materials Mater. Res. Soc. Symp. Proc. 115 MRS Pittsburgh PA. (Number I in the series.) We’ve updated the flow chart in the article on p51 by Goodhew, PJ, The tripod polisher is described by Klepeis, SJ, Benedict, JP and Anderson, RM on p179. (Pictures of the gem variety are shown in Figure 36.3 of Ceramic Materials by Carter and Norton.) Brown, JM and Sheng, TJ describe the use of lithography on p229.Google Scholar
  3. ii. Anderson, RM (Ed.) 1990 Specimen Preparation for Transmission Electron Microscopy of Materials, II Mater. Res. Soc. Symp. Proc. 199 MRS Pittsburgh PA.Google Scholar
  4. iii. Anderson, RM, Tracy, B and Bravman, JC (Eds.) 1992 Specimen Preparation for Transmission Electron Microscopy of Materials, III Mater. Res. Soc. Symp. Proc. 254 MRS Pittsburgh PA. Alani, R and Swann, PR (1992) discuss ion milling on p43.Google Scholar
  5. iv. Anderson, RM and Walck, SD (Eds.) 1997 Specimen Preparation for Transmission Electron Microscopy of Materials, IV Mater. Res. Soc. Symp. Proc. 480 MRS Pittsburgh PA.Google Scholar

Chemical Polishing

  1. Thompson-Russell, KC and Edington, JW (1977) Electron Microscope Specimen Preparation Techniques in Materials Science Macmillan Philips Technical Library Eindhoven Netherlands. Many recipes.Google Scholar

Ion Milling and Fib

  1. Barber, DJ 1970 Thin Foils of Non-metals Made for Electron Microscopy by Sputter-Etching J. Mater. Sci. 5(1) 1–8. First use of ion milling to make a ceramic TEM sample.Google Scholar
  2. Barna, A 1992 Topographic Kinetics and Practice of Low Angle Ion Beam Thinning in MRS Proc. 254 3–22. An early advocate of using low-energy ion beams.Google Scholar
  3. Cullis, AG, Chew, NG and Hutchinson, JL 1985 Formation and Elimination of Surface Ion Milling Defects in Cadmium Telluride, Zinc Sulphide and Zinc Selenide Ultramicroscopy 17 203–211. The paper on reactive-ion milling of TEM samples.Google Scholar
  4. Giannuzzi, LA and Stevie, FA 2004 Introduction to Focused Ion Beams: Instrumentation, Theory, Techniques and Practice Springer Verlag NY. The guide to FIB.Google Scholar
  5. Harriott, LR 1991 The Technology of Finely Focused Ion Beams Nucl. Instr. Meth. Phys. Res. Section B: Beam Interactions with Materials and Atoms 55B (1–4) 802–810. One place to start if you’re interested in ‘Why Ga?’Google Scholar
  6. Medard, L, Jacquet, PA and Sartorius, R 1949 Sur les dangers d'explosion des bains aceto-perchloriques de polissage electrolytique (Explosion Hazard of Acetic and Perchloric Acid Mixture Used as Solution in Electrolytic Polishing) Rev. Metall. 46(8) 549–560. Jacquet has many other papers on specimen preparation if your French is good.Google Scholar

Other Materials

  1. Carter, CB and Norton, MG 2007 give some illustrations of the tripod polisher used to facet diamond in Ceramic Materials: Science and Engineering Springer Verlag NY.Google Scholar
  2. Malis, TF 1989 AEM Specimens: Staying One Step Ahead in Microbeam Analysis-1989 487–490 Ed. P.E. Russell, San Francisco Press San Francisco gives a discussion of using the microtome for hard samples.Google Scholar
  3. Sawyer, LC, Grubb, DT and Meyers, GF 2008 Polymer Microscopy 3rd Ed. Springer Verlag NY gives the details for preparing polymer specimens.Google Scholar

Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  1. 1.The University of Alabama in HuntsvilleHuntsvilleUSA
  2. 2.University of ConnecticutStorrsUSA

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